Synthese, Struktur und thermisches Verhalten von Thiophosphorsäuretriamid SP(NH2)3 [1] / Synthesis, Structure, and Thermal Behaviour of Phosphorothionic Triamide SP(ΝΗ2)3 [1]

1989 ◽  
Vol 44 (8) ◽  
pp. 942-945 ◽  
Author(s):  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Thermal Properties ◽  
Single Crystal ◽  
Melting Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Ray Methods ◽  
Single Bonds

Phosphorothionic triamide SP(NH2)3 is obtained by slow addition of SPCl3 dissolved in dry CH2Cl2 to a satured solution of NH3 in CH2Cl2 at —50°C. Ammonium chloride is removed from the resulting precipitate by treatment with HNEt2 followed by extraction with CH2Cl2. Coarse crystalline SP(NH2)3 is obtained after recrystallization from dry methanol. The crystal structure of SP(NH2)3 has been determined by single crystal X-ray methods (Pbca; a = 922.3(1), b = 953.8(1), c = 1058.4(2) pm, Z = 8). In the crystals the molecules show non-crystallographic point symmetry C8. The P—S bond (195.4(1) pm) is slightly longer than in SPCl3. From P—N bond lengths of about 166 pm a significant electrostatic strengthening of the P—N single bonds is assumed. Weak intermolecular hydrogen bonding interactions (N —H · · · N ≥ 329.5 pm; N — H · · · S ≥ 348.3 pm) are observed.Investigation of thermal properties shows a melting temperature of 115°C for SP(NH2)3. According to combined DTA/TG and MS investigations above this temperature the compound decomposes by evolution of H2S and NH3 to yield amorphous phosphorus(V)nitride.

Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaamino-1-oxo- 1λ5 ,3λ5-diphosphaz-2-en, (NH2)2(O)P-N=P(NH2)3 / Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaamino-1-oxo-1λ5, 3λ5-diphosphaz-2-ene, (NH2)2(O)P-N=P(NH2)3

1996 ◽  
Vol 51 (8) ◽  
pp. 1079-1083 ◽  
Author(s):  
N. Stock ◽  
W. Schnick
Keyword(s):  
Crystal Structure ◽  
Thermal Properties ◽  
Room Temperature ◽  
Three Dimensional ◽  
Intermolecular Hydrogen Bonding ◽  
Structure And Properties ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network ◽  
Ray Methods

Coarse crystalline (NH2)2(O)P-N=P(NH2)3 is obtained from a NH3 saturated CH2Cl2 suspension of (NH2)2(O)P-N=P(NH2)3 NH4Cl at room temperature. (NH2)2(O)P-N=P(NH2)3·NH4Cl is synthesized by slow addition of Cl2(O)P-N=PCl3 to a solution of NH3 in CH2Cl2 at -78 °C. Excess NH4Cl is removed by treatment with HNEt2 followed by extraction with CH2Cl2. The crystal structure of (NH2)2(O)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c; a = 1462.8(3), b = 944.8(2), c = 1026.9(2) pm, β = 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H···N ≥ 313 pm. N-H···O ≥ 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80 °C.

Study on Novel Structure of Praseodymium Complex, C5H13O11Pr

2013 ◽  
Vol 834-836 ◽  
pp. 515-518
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Ting Ting Huang ◽  
Yang Xu ◽  
Lin Tong Wang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Hydrothermal Reaction ◽  
Crystal Packing ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Novel Structure ◽  
Praseodymium Complex

A novel praseodymium complex C5H13O11Pr has been synthesized from hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Pr1 atom is nine coordinated by nine O atoms. The crystal packing is stabilized by O-H...O hydrogen bonding interactions.

Synthesis of Glycolic and Oxalic Acid Europium: [Eu (C3 H6O9)] ·2(H2O)

2012 ◽  
Vol 554-556 ◽  
pp. 792-795
Author(s):  
Hai Xing Liu ◽  
Jing Wang ◽  
Fang Fang Jian ◽  
Hui Juan Yue ◽  
Guang Zeng ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Oxalic Acid ◽  
Single Crystal ◽  
Hydrothermal Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
The Eu

A new Eu complex [Eu (C3O9H6)] ·2(H2O) has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Eu atom is coordinated by eight O atoms. The molecular is antisymmetric structure by the C3-C3 axis. It is striking that the structure of the complex exhibits extensive O-H…O hydrogen-bonding interactions.

Study on a Novel Structure of Yttrium Complex, C4H10O10Y

2013 ◽  
Vol 785-786 ◽  
pp. 424-427
Author(s):  
Hai Xing Liu ◽  
Qing Hua Zhang ◽  
Zhang Xue Yu ◽  
Quan Hua Fan ◽  
Ting Ting Huang ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Hydrothermal Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Novel Structure

The Y complex C4H10O10Y has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Y atom is coordinated by nine O atoms. The molecular structure stabilized by the O-H…O hydrogen-bonding interactions.

scholarly journals Redetermination of ammonium metavanadate

IUCrData ◽  
2018 ◽  
Vol 3 (8) ◽  
Author(s):  
Aarón Pérez-Benítez ◽  
Sylvain Bernès
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Single Crystal ◽  
Structural Data ◽  
Ammonium Cation ◽  
Ammonium Metavanadate ◽  
Starting Material ◽  
X Ray ◽  
Hydrogen Bonding Interactions

The crystal structure of ammonium metavanadate, NH4VO3, a compound widely used as a starting material for the synthesis of vanadium and polyoxidovanadate compounds, had been determined twice using single-crystal X-ray data [Syneček & Hanic (1954). Czech. J. Phys. 4, 120–129 (Weissenberg data); Hawthorne & Calvo (1977). J. Solid State Chem. 22, 157–170 (four-circle diffractometer data)]. Its structure is now redetermined at higher resolution using Ag Kα radiation, and the result is compared with the former refinements. Structural data for the polymeric [VO3]∞ chain remain unchanged, while more accurate parameters are obtained for the ammonium cation, improving the description of hydrogen-bonding interactions in the crystal structure.

Study on a Structure of 2,6-Pyridine Dicarboxylic Acid Gallium, (NH4)Ga(C7H3NO4)2

2013 ◽  
Vol 470 ◽  
pp. 3-6
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Xiao Ri Sun ◽  
Lin Tong Wang ◽  
Yun Chen Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Dicarboxylic Acid ◽  
Crystal Packing ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Pyridine Dicarboxylic Acid ◽  
Solution Reaction

A novel Ga complex (NH4)Ga(C7H3NO4)2 has been synthesized from a solution reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Ga atom is six-coordinated by two N atoms and four O atoms from two 2,6-pyridine dicarboxylic acid anions. The crystal packing is stabilized by O-H...N hydrogen bonding interactions.

Group 15 Metal Complexes With Carboxylic Acids. Preparation and Crystal Structure of Polymeric Ammonium Aquabis[(+)-tartrato(2-)]bismuthate(III) Hydrate

1992 ◽  
Vol 45 (6) ◽  
pp. 1027 ◽  
Author(s):  
DS Sagatys ◽  
EJ Oreilly ◽  
S Patel ◽  
RC Bott ◽  
DE Lynch ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Metal Complexes ◽  
Tartaric Acid ◽  
Carboxylic Acids ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
A Cell ◽  
Ray Methods

The crystal structure of the bismuth(III) complex with (+)-tartaric acid, ammonium aquabis [(+)-tartrato (2-)] bismuthate (III) hydrate, has been determined by X-ray methods and refined to a residual R 0.020 for 1288 observed reflections. Crystals are orthorhombic, space group P 212121 with Z 4 in a cell of dimensions a 7.4712(4), b 10.856(1), c 17.609(3) � . Each nine-coordinate MO9 bismuth centre comprises three bidentate α-hydroxy carboxy residues from two tartrato (2-) ligands (with one bridging), an asymmetric bidentate carboxylato (O,O') group, and a water. The Bi-O range is 2.372(7)-2.738(6) � [mean 2.509(6) >� ]. The resultant structure is a linear polymer which is stabilized by extensive hydrogen-bonding interactions.

Synthesis, crystal structure of the simultaneous binding of Ni(II) cation and chloride by the protonated 2,4,6 tris-(2-pyridyl)-1,3,5 triazine ligand: Theoretical investigations of anion···π, π···π and hydrogen bonding interactions

2021 ◽  
Author(s):  
Pampi Pal ◽  
kinsuk das ◽  
Anowar Hossain ◽  
Rosa Maria Gomila ◽  
Antonio Frontera ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Theoretical Investigations ◽  
Protonated Ligand

A new octahedral Ni(II) complex 1 of protonated ligand Htptz+ (tptz: 2,4,6-tris(2-pyridyl)-1,3,5-triazine) has been synthesized and characterized by single crystal X-ray analysis. It is worth of note that the protonated...

Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumiodid [P(NH2)4]I / Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Iodide [P(NH2)4]I

1994 ◽  
Vol 49 (10) ◽  
pp. 1381-1386 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Room Temperature ◽  
Bond Distance ◽  
Acetonitrile Solution ◽  
Structure And Properties ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Anions And Cations ◽  
Ray Methods

Abstract The title compound has been prepared starting from phosphorothionic triamide SP(NH2)3 by methylation of the sulfur atom and subsequent ammonolysis reaction in dry acetonitrile and dichloromethane, respectively, both at room temperature. Suitable single crystals are obtained from an acetonitrile solution in a temperature gradient between 70 °C and room temperature. The crystal structure of [P(NH2)4]I has been determined by single crystal X-ray methods (P4/nbm; a = 842.6(2), c = 486.7(2) pm, Z = 2). In the solid [P(NH2)4]+ - and I−-ions are found with significant N - H···I-hydrogen bonding interactions between anions and cations (H -I: 276.4 pm). The P - N - bond length in the cation (160.7(2) pm) represents the shortest P - NH2 bond distance reported to date indicating a significant electrostatic strengthening. The condensation behaviour of [P(NH2)4]I in solution and in the solid has been investigated.

Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaaminol- 1-thio-1 λ5,3λ5-diphosphaz-2-en (NH2)2P(S)N=P(NH2)3 / Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaam 1-thio-1 λ5,3λ5-diphosphaz-2-en (NH2)2P(S)N=P(NH2)3

1997 ◽  
Vol 52 (4) ◽  
pp. 490-495 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Hydrogen Atom ◽  
Room Temperature ◽  
Acetonitrile Solution ◽  
Structure And Properties ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Ray Methods

Abstract (NH2)2P(S)N=P(NH2)3 has been prepared by a two step synthesis. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of (NH2)2P(S)N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c, a = 998.27(9) b = 762.78(8), c = 1007.70(15) pm, β = 107.340(7)°, Z = 4). In the crystal structure each hydrogen atom is subject to a hydrogen bond. Four N-H -N hydrogen bonding interactions per molecule build up a framework connecting two molecules in eight-membered rings. Each sulfur atom shows six distances N-H···S in the range of weak hydrogen bonding interactions.

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